CN103551589B - The synthetic method of flower-shaped silver-colored micron particles - Google Patents
The synthetic method of flower-shaped silver-colored micron particles Download PDFInfo
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- 239000002245 particle Substances 0.000 title claims abstract description 40
- 238000010189 synthetic method Methods 0.000 title claims abstract description 20
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims abstract description 76
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 56
- 229960005070 ascorbic acid Drugs 0.000 claims abstract description 37
- 235000010323 ascorbic acid Nutrition 0.000 claims abstract description 37
- 239000011668 ascorbic acid Substances 0.000 claims abstract description 37
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 31
- 239000010935 stainless steel Substances 0.000 claims abstract description 31
- 239000000758 substrate Substances 0.000 claims abstract description 31
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 23
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000243 solution Substances 0.000 claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims abstract description 9
- 238000005119 centrifugation Methods 0.000 claims abstract description 8
- 239000000843 powder Substances 0.000 claims abstract description 8
- 238000013019 agitation Methods 0.000 claims abstract description 7
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 239000002244 precipitate Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000012634 fragment Substances 0.000 claims description 4
- 239000000047 product Substances 0.000 abstract description 15
- 238000002360 preparation method Methods 0.000 abstract description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 18
- 238000003756 stirring Methods 0.000 description 17
- 229910052709 silver Inorganic materials 0.000 description 11
- 239000004332 silver Substances 0.000 description 11
- 238000004090 dissolution Methods 0.000 description 8
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000003638 chemical reducing agent Substances 0.000 description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000002073 nanorod Substances 0.000 description 3
- 238000006555 catalytic reaction Methods 0.000 description 2
- 239000008139 complexing agent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 239000002923 metal particle Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 150000007524 organic acids Chemical class 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- ODIGIKRIUKFKHP-UHFFFAOYSA-N (n-propan-2-yloxycarbonylanilino) acetate Chemical compound CC(C)OC(=O)N(OC(C)=O)C1=CC=CC=C1 ODIGIKRIUKFKHP-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 240000004922 Vigna radiata Species 0.000 description 1
- 235000010721 Vigna radiata var radiata Nutrition 0.000 description 1
- 235000011469 Vigna radiata var sublobata Nutrition 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000000138 intercalating agent Substances 0.000 description 1
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 1
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 1
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 description 1
- 229940038773 trisodium citrate Drugs 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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Abstract
The invention discloses a kind of synthetic method of flower-shaped silver-colored micron particles, take ascorbic acid pressed powder and silver nitrate crystal first respectively, it is dissolved respectively in deionized water stand-by; Add in liquor argenti nitratis ophthalmicus by the ascorbic acid solution of configuration, the mol ratio of ascorbic acid and silver nitrate is 0.8 ~ 1.2: 1; Finish the stainless steel substrates adding in mixed solution immediately and cleaned up; Stainless steel substrates adds rear to reaction mass magnetic agitation 180min ~ 360min, and reaction terminates; Centrifugation after stainless steel substrates in material after reaction terminates takes out, after washing of precipitate, drying obtains flower-shaped silver-colored micron particles.Preparation method of the present invention is to the morphology controllable of product, simple to operate, mild condition and reproducible.
Description
Technical field
The pattern that the present invention relates to Argent grain controls synthetic method, is specifically related to a kind of synthetic method of flower-shaped silver-colored micron particles.
Background technology
Silver has the characteristics such as unique catalysis, antibacterial, nonlinear optics and conductive and heat-conductive, has broad application prospects in fields such as inorganic antiseptic, catalysis material, electrocondution slurries.The character of silver and application are all strongly depend on size and the pattern of Argent grain.The silver at present with difformity, size and structure is synthesized out.
Nano metal particles has reunion and arch formation, and its nano effect and specific area are restricted.Flower-like structure can effectively be avoided reuniting and arch formation, has the characteristic of high surface, high reaction activity.
About the synthetic method of flower-shaped silver-colored structural material, Chinese patent literature CN 103273082 A discloses a kind of preparation method of flower-like spherical silver powder, and configure liquor argenti nitratis ophthalmicus and reductant solution respectively, described reductant solution is copperas solution; In liquor argenti nitratis ophthalmicus, add complexing agent, described complexing agent is at least one of acylate of more than the organic acid anhydride of more than the organic acid of more than binary and binary, binary and binary and binary and binary; Liquor argenti nitratis ophthalmicus and reductant solution are cooled to 0 DEG C ~ 20 DEG C; Joined by reducing agent in liquor argenti nitratis ophthalmicus, constantly stir until solution colour no longer changes, reaction stops; After centrifugation or natural subsidence, wash successively with deionized water and absolute ethyl alcohol, after vacuum drying, obtain the flower-like spherical silver powder of particle diameter 0.5 ~ 3 μm of scope.
Hydro-thermal method is adopted in the Master's thesis " preparation of multi-morphology nano silver and controllability Study thereof " that Central South University's sun element is beautiful, under surface dispersant PVP exists, with ascorbic acid reduction silver nitrate, synthesize the flower-like nanometer silver self-assembled structures that size dimension is about 1 ~ 2 μm, its basic cell structure is by diameter about 120nm, and the Silver nanorod that length is approximately about 1 μm evenly assembles.Optimum experimental condition is: reaction temperature 150 DEG C, and the reaction time is 10h, and silver nitrate concentration 9.968mM, AsA concentration is 9.968mM, PVP concentration is 0.171mM.
Zhang Bo equals to be published in " synthesis of flower-shaped silver-colored micro nano structure and the SERS character " literary composition on " SCI " method providing and prepare the flower-shaped silver-colored micro nano structure be made up of nanometer sheet in system that a kind of nitric acid adjust ph and trisodium citrate coexist with ascorbic acid reduction silver nitrate in August, 2010.This preparation method uses citric acid as intercalating agent, uses red fuming nitric acid (RFNA) adjust ph, only has when the pH value of solution is about 3.5 time, just can obtain the silver-colored micro nano structure of good pattern, have corrosivity, operate comparatively loaded down with trivial details.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of synthetic method of simple to operate, reaction condition is gentle, the reaction time is short flower-shaped silver-colored micron particles.
The technical scheme realizing the object of the invention is a kind of synthetic method of flower-shaped silver-colored micron particles, comprises the following steps:
1. take ascorbic acid pressed powder and silver nitrate crystal respectively, it is dissolved respectively in deionized water stand-by.
2. the ascorbic acid solution that 1. step configures is added in liquor argenti nitratis ophthalmicus, finish the stainless steel substrates adding in mixed solution immediately and cleaned up; The mol ratio of ascorbic acid and silver nitrate is 0.8 ~ 1.2: 1; Stainless steel substrates adds rear to reaction mass magnetic agitation 180min ~ 360min, and reaction terminates.
3. centrifugation after stainless steel substrates step 2. reacted in the material after terminating takes out, after washing of precipitate, drying obtains flower-shaped silver-colored micron particles.
Optionally, above-mentioned steps 2. stainless steel substrates add and in reaction mass, pass into air with micropump to while reaction mass magnetic agitation afterwards.
Preferably, the concentration of liquor argenti nitratis ophthalmicus that 1. step configures is 0.5 mol/L ~ 0.75mol/L.
Preferably, the concentration of ascorbic acid solution that 1. step configures is 0.5 mol/L ~ 0.70mol/L.
The stainless steel substrates that 2. above-mentioned steps adds is 201,202,301,304,316,631,321,430 or 410 stainless steel substrates.
Preferably, step 2. the addition of stainless steel substrates be add 0.1g ~ 5g in every 20mL reaction solution; Stainless steel substrates adds after being cut into fragment.
The present invention has positive effect: the method for the flower-shaped silver of (1) synthesis of the present invention adopts ascorbic acid to reduce silver nitrate as reducing agent, aqueous ascorbic acid is joined after in liquor argenti nitratis ophthalmicus and add stainless steel substrates immediately, under the environment that stainless steel substrates exists, silver nitrate is reduced, and the silver obtained has floriform appearance.
(2) preparation method of the present invention is to the morphology controllable of product, simple to operate, mild condition and reproducible.
Accompanying drawing explanation
Fig. 1 is the SEM photo of flower-shaped silver-colored micron particles prepared by embodiment 1;
Fig. 2 is the SEM photo of flower-shaped silver-colored micron particles prepared by embodiment 2;
Fig. 3 is the SEM photo of flower-shaped silver-colored micron particles prepared by embodiment 3;
Fig. 4 is the SEM photo of flower-shaped silver-colored micron particles prepared by embodiment 4;
Fig. 5 is the SEM photo of flower-shaped silver-colored micron particles prepared by embodiment 5;
Fig. 6 is the SEM photo of flower-shaped silver-colored micron particles prepared by embodiment 6;
Fig. 7 is the SEM photo of flower-shaped silver-colored micron particles prepared by embodiment 7;
Fig. 8 is the SEM photo of flower-shaped silver-colored micron particles prepared by embodiment 8.
Detailed description of the invention
(embodiment 1)
The synthetic method of the flower-shaped silver-colored micron particles of the present embodiment comprises the following steps:
1. take 1.0004g(0.005680 mol) ascorbic acid (No. CAS: 50-81-7)) white solid powder join in the beaker filling 10mL deionized water, stir make dissolution of ascorbic acid stand-by, the concentration of ascorbic acid solution is 0.5680mol/L.
The crystal taking 0.9987g silver nitrate (0.005879mol) joins in 10mL deionized water, and stir and make silver nitrate dissolving stand-by, the concentration of liquor argenti nitratis ophthalmicus is 0.5879 mol/L.
The mol ratio of ascorbic acid and silver nitrate preferably controls 0.8 ~ 1.2: 1, is 0.97: 1 in the present embodiment.
The concentration of ascorbic acid solution preferably controls at 0.5 mol/L ~ 0.7 mol/L; The concentration of liquor argenti nitratis ophthalmicus preferably controls at 0.5 mol/L ~ 0.75mol/L.
2. the ascorbic acid solution that 1. step configures is added in liquor argenti nitratis ophthalmicus, finish the 201 stainless steel substrates 1.6021g adding in mixed solution immediately and cleaned up; Stainless steel substrates add rear in reaction mass magnetic agitation 180min ~ 360min(the present embodiment for 240min), reaction terminates.Reaction temperature is 0 DEG C ~ 50 DEG C, preferably 20 DEG C ~ 40 DEG C.
The stainless steel substrates added adds after being cut into fragment by the stainless steel substrates of full wafer, and in the present embodiment, fragment is about mung bean size.
3. 201 stainless steel substrates step 2. reacted in the material after terminating take out with clean tweezers, and the 201 stainless steel substrates 5mL deionized water rinsing of taking-up, flushing liquor is incorporated in reacted material.
To take out the reacted material centrifugation of stainless steel substrates, the precipitate with deionized water that centrifugation obtains washs 10 times, and the product after washing is dry at nitrogen atmosphere 50 DEG C.Obtain silver powder 0.6203g, productive rate 97.78%.
The pattern of product and the observation of granularity are carried out under S-3400NII type (Japanese Hitachi company produces) SEM (SEM), and following embodiment and comparative example all adopt this instrument to carry out the observation of pattern and granularity.
The SEM of product the results are shown in Figure 1, and product has more homogeneous pattern, good dispersion.The SEM photo display particle of powder is rose-shaped, and the particle diameter of particle is at about 2 μm; And " petal " of described flower-shaped silver-colored micron particles by diameter 0.25 μm, length is that the Silver nanorod of about 2.5 μm evenly assembles.
The silver of flower-like structure effectively can avoid reunion and the arch formation of nano metal particles, has the characteristic of high surface, high reaction activity.
(embodiment 2)
All the other are identical with embodiment 1 for the synthetic method of the flower-shaped silver-colored micron particles of the present embodiment, and difference is:
Step 1. in 1.0006g ascorbic acid is joined in 10ml deionized water, stir make dissolution of ascorbic acid; 0.9985g silver nitrate crystal is joined in 10ml deionized water, stir and silver nitrate is dissolved.
Step 2. in ascorbic acid solution that 1. step is configured add in liquor argenti nitratis ophthalmicus, finish the 201 stainless steel substrates 1.6021g adding in mixed solution immediately and cleaned up; In reaction mass, pass into air with micropump while reaction mass magnetic agitation, after 240min, reaction terminates.Air mass flow is 8mL/min.
The SEM of product the results are shown in Figure 2, and product has more homogeneous pattern, good dispersion.The SEM photo display particle of powder is rose-shaped, and the particle diameter of particle is at about 3 μm; And " petal " of described flower-shaped silver-colored micron particles by diameter 0.25 μm, length is that the Silver nanorod of about 2.5 μm evenly assembles.
Except 201 stainless steel substrates that the present embodiment is used, also can add 202,301,304,316,631,321,430 or 410 stainless steel substrates in reaction solution; Obtained powder SEM photo display particle is also rose-shaped.
(comparative example 1)
The synthetic method of the flower-shaped silver-colored micron particles of this comparative example comprises the following steps:
1. take 0.9698g ascorbic acid (No. CAS: 50-81-7)) white solid powder join in the beaker filling 10mL deionized water, stir make dissolution of ascorbic acid stand-by.
The crystal taking 0.9991g silver nitrate joins in 10mL deionized water, stirs and makes silver nitrate dissolving stand-by.
2. add in liquor argenti nitratis ophthalmicus by the ascorbic acid solution that 1. step configures, leave standstill reaction 240min, reaction terminates.
3. 2. step is reacted the material centrifugation after terminating, the precipitate with deionized water that centrifugation obtains washs 10 times, and the product after washing is dry at nitrogen atmosphere 50 DEG C.
The SEM of product the results are shown in Figure 3, the irregular silver particles of to be size the be 300nm ~ 600nm obtained.
(comparative example 2)
All the other are identical with comparative example 1 for the synthetic method of the flower-shaped silver-colored micron particles of this comparative example, and difference is:
Step 1. in 1.0012g ascorbic acid is joined in 50ml deionized water, stir make dissolution of ascorbic acid; 0.9976g silver nitrate crystal is joined in 50ml deionized water, stir and silver nitrate is dissolved.
The SEM of product the results are shown in Figure 4, to be size the be flower-shaped Argent grain of class of about 2.4 μm obtained.
(comparative example 3)
All the other are identical with comparative example 1 for the synthetic method of the flower-shaped silver-colored micron particles of this comparative example, and difference is:
Step 1. in 1.0010g ascorbic acid is joined in 100ml deionized water, stir make dissolution of ascorbic acid; 0.9926g silver nitrate crystal is joined in 100ml deionized water, stir and silver nitrate is dissolved.
The SEM of product the results are shown in Figure 5, to be size the be flower-shaped Argent grain of class of about 4 μm obtained.
(comparative example 4)
All the other are identical with comparative example 1 for the synthetic method of the flower-shaped silver-colored micron particles of this comparative example, and difference is:
Step 1. in 1.0007g ascorbic acid is joined in 10ml deionized water, stir make dissolution of ascorbic acid; 0.9985g silver nitrate crystal is joined in 10ml deionized water, stir and silver nitrate is dissolved.
The SEM of product the results are shown in Figure 6, to be size the be flower-shaped Argent grain of class of about 1 μm obtained.
(comparative example 5)
All the other are identical with comparative example 1 for the synthetic method of the flower-shaped silver-colored micron particles of this comparative example, and difference is:
Step 1. in 1.0006g ascorbic acid is joined in 20ml deionized water, stir make dissolution of ascorbic acid; 0.9982g silver nitrate crystal is joined in 20ml deionized water, stir and silver nitrate is dissolved.
The SEM of product the results are shown in Figure 7, to be size the be flower-shaped Argent grain of class of 1 μm ~ 2 μm obtained.
(comparative example 6)
All the other are identical with comparative example 1 for the synthetic method of the flower-shaped silver-colored micron particles of this comparative example, and difference is:
Step 1. in 1.0001g ascorbic acid is joined in 100ml deionized water, stir make dissolution of ascorbic acid; 0.9986g silver nitrate crystal is joined in 100ml deionized water, stir and silver nitrate is dissolved.
The SEM of product the results are shown in Figure 8, to be size the be flower-shaped Argent grain of class of about 1.2 μm obtained.
Claims (4)
1. a synthetic method for flower-shaped silver-colored micron particles, is characterized in that comprising the following steps:
1. take ascorbic acid pressed powder and silver nitrate crystal respectively, it is dissolved respectively in deionized water stand-by; The concentration of the ascorbic acid solution of configuration is 0.5 mol/L ~ 0.70mol/L, and the concentration of the liquor argenti nitratis ophthalmicus of configuration is 0.5 mol/L ~ 0.75mol/L;
2. the ascorbic acid solution that 1. step configures is added in liquor argenti nitratis ophthalmicus, finish the stainless steel substrates adding in mixed solution immediately and cleaned up; The addition of stainless steel substrates is add 0.1g ~ 5g in every 20mL reaction solution; The mol ratio of ascorbic acid and silver nitrate is 0.8 ~ 1.2: 1; Stainless steel substrates adds rear to reaction mass magnetic agitation 180min ~ 360min, and reaction terminates;
3. centrifugation after stainless steel substrates step 2. reacted in the material after terminating takes out, after washing of precipitate, drying obtains flower-shaped silver-colored micron particles.
2. the synthetic method of flower-shaped silver-colored micron particles according to claim 1, is characterized in that: step 2. stainless steel substrates adds and in reaction mass, passes into air with micropump to while reaction mass magnetic agitation afterwards.
3. the synthetic method of flower-shaped silver-colored micron particles according to claim 1 and 2, is characterized in that: the stainless steel substrates that 2. step adds is 201,202,301,304,316,631,321,430 or 410 stainless steel substrates.
4. the synthetic method of flower-shaped silver-colored micron particles according to claim 3, is characterized in that: stainless steel substrates adds after being cut into fragment.
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| CN103909257B (en) * | 2014-03-21 | 2016-04-13 | 中科院广州化学有限公司南雄材料生产基地 | A kind of spike structure nano silver line and electrically-conducting paint thereof and preparation and application |
| CN106493385B (en) * | 2016-10-25 | 2018-06-15 | 中国科学院合肥物质科学研究院 | The preparation method of silver-colored triangular nano piece |
| CN106770159A (en) * | 2016-12-02 | 2017-05-31 | 中国计量大学 | High sensitivity food color detection method |
| CN108031864B (en) * | 2018-01-23 | 2020-09-01 | 电子科技大学 | Preparation method of nano silver wire cluster with antibacterial activity |
| CN109382512A (en) * | 2018-12-07 | 2019-02-26 | 五邑大学 | A kind of preparation method of flower-like nanometer aluminium powder self-assembled structures |
| CN109773210A (en) * | 2019-03-01 | 2019-05-21 | 天津工业大学 | A kind of preparation method of the flower shape micro-silver powder with elongated big petal |
| CN109807348A (en) * | 2019-03-01 | 2019-05-28 | 淮海工学院 | A kind of simple environment-friendly preparation method thereof of micro-nano silver |
| CN111804931A (en) * | 2019-04-11 | 2020-10-23 | 香港大学 | Antibacterial stainless steel prepared by powder metallurgy method assisted by in-situ decomposition |
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| CN111673090B (en) * | 2020-06-09 | 2022-12-20 | 中北大学 | Preparation method of flower-like silver by using gallic acid as structure-directing agent |
| CN112126416A (en) * | 2020-10-14 | 2020-12-25 | 北京工业大学 | Microfluidic synthesis method and device for silver nanofluid |
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Also Published As
| Publication number | Publication date |
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| CN104985190A (en) | 2015-10-21 |
| CN104985190B (en) | 2017-06-13 |
| CN103551589A (en) | 2014-02-05 |
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